HRID564494
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
3-[({[1,6-Diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}amino)carbonyl]benzoic acid (0.451 g, 1 mmol), [(3-bromo-4-methylphenyl)methyl]amine (0.2 g, 1 mmol, HBTU (0.379 g, 1 mmol), and TEA (0.278 mL, 2 mmol) were combined in CH2Cl2 (25 mL). The mixture was stirred overnight at room temperature. Aqueous workup gave the crude product which was CombiFlashed on a 40 g column eluted with 0-10% MeOH/CH2Cl2 to give the title compound as a white solid. LC-MS m/z 633.8 (M+H)+, 1.85 min (ret time); mp 175-176° C.; analytical HPLC shows 97.5% purity, (ret time 13.568 min).
WORKUP
后处理
- customAqueous workup gave the crude product which
- washeluted with 0-10% MeOH/CH2Cl2